CN105671514B - A kind of method that two-step method prepares porous iridium - Google Patents
A kind of method that two-step method prepares porous iridium Download PDFInfo
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- CN105671514B CN105671514B CN201610202922.XA CN201610202922A CN105671514B CN 105671514 B CN105671514 B CN 105671514B CN 201610202922 A CN201610202922 A CN 201610202922A CN 105671514 B CN105671514 B CN 105671514B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
- C23C16/18—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metallo-organic compounds
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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Abstract
The invention belongs to a kind of preparation field of porous material, specifically discloses a kind of method that " chemical vapor deposition "+" high-temperature roasting " two-step method prepares porous iridium.The first step is " method of chemical vapor deposition prepares iridium "：The matrix of selection is molybdenum, can improve deposition quality using coreaction gas.After obtaining being deposited on the iridium on Mo substrate, matrix is eroded using suitable corrosive agent, obtains metal iridium.Second step is " method of high-temperature roasting prepares porous iridium "：High-temperature roasting is carried out under high temperature, protective atmosphere to iridium, obtains porous iridium.Because porous iridium fusing point is high, fragility is big, and it is more difficult that conventional method prepares porous iridium, of the invention by the way of high-temperature roasting after chemical vapor deposition, obtains porous iridium, technological process is relatively simple, porosity, and average pore size can control.
Description
Technical field
The present invention relates to a kind of method that two-step method prepares porous iridium, belong to the preparing technical field of porous metal material,
A kind of method for preparing porous iridium more particularly to " chemical vapor deposition "+" high-temperature roasting " two-step method.
Background technology
Porous metal material is to develop a kind of more rapid material in present material science, and its specific surface area is big, density
It is small, it is widely used.As functional material, available for porous metals filtering material, catalyst and electrode material.
However, the outstanding properties problem of current porous metals filtering material is corrosion-resistant and insufficient (the yellow state of resistance to elevated temperatures
Great waves, Zuo Xiaoqing, Sun Yanlin, Zhou Yun, Lu Jiansheng, Wang Hong porous metals filtering material progress [J] material Leaders, 2010,
S2:448-452+456.).And precious metal iridium, fusing point is high, antioxygenic property is good, prepares porous iridium as metallic filter material,
It can solve the above problems.
Iridium is also widely used in organic reaction catalyst, and (preparation, sign and its performance of Zhang Xiongwei precious metal iridium catalyst are ground
Study carefully [D] Sichuan Universitys, 2005.) and electrode material (Chen Dongchu, Zheng family's Son, pays Chaoyang .H+The research of electrodes selective material is entered
Exhibition [J] Arms Material scientific and engineerings, 2004,02:67-71.).For catalyst and electrode material, the weight of its performance is determined
It is specific surface area to want parameter, prepares porous iridium, can significantly lift its specific surface area.
Therefore, porous iridium is prepared, there is realistic meaning.The currently known method for preparing porous material has：
(1) liquid phase method：1. direct foaming：By being blown to the molten metal for adding tackifier, foam metal is prepared；Or
By adding foaming agent (metal hydride powder) in molten metal bath, foaming agent is produced hydrogen by thermal decomposition, cause body
Product expands and makes metal foaming.2. casting：By making the core of " foaming ", core is recycled to be cast, finally by
Method removes core, obtains porous metals.
(2) solid phase method：1. powder metallurgic method：Using pore creating material and powder pressing forming, then sinter, finally by method
Remove pore creating material.2. first deposited metal obtains metal ball on organic polymer ball, then removes organic polymer ball by method
Obtain hollow metal high score bulbec.Most a large amount of metal-polymer balls are sintered together at last.
(3) sedimentation：Deposited on the surface of foams by the method or CVD method of electrochemistry.
But liquid phase method is primarily adapted for use in the metal of low melting point, such as Al, Mg, Zn.For refractory metal, frequently with powder
Metallurgical and sedimentation, dependent on pore creating material or foams, its technological process is more complicated, and technological parameter is difficult to control.And noble metal
Iridium, more because fusing point is high, fragility is big, and the difficulty for preparing porous iridium is bigger.
The content of the invention
The invention aims to propose that a kind of utilization " chemical vapor deposition "+" high-temperature roasting " prepares the two of porous iridium
Footwork.
Technical scheme is as follows：
A kind of method that two-step method prepares porous iridium, steps of the method are：
(1) chemical vapour deposition technique (MOCVD) prepares iridium (Ir)：
The preparation that the present invention carries out Ir by MOCVD methods is with Ir (acac)3For presoma, original work are gone back by hydrogen
With using argon gas as carrier gas, depositing to form Ir coatings in Mo matrix surfaces.Its fundamental reaction principle is：
Ir(acac)3+H2→Ir(s)+CxHyOz(g)(CxHyOzFor admixture of gas)
Its operation is as follows：
A. Mo substrate is put into ethanol after blasting treatment and is cleaned by ultrasonic, scavenging period 10min, after cleaning
Matrix is put into baking oven and dried；
B. SiC sand and Ir (acac) are weighed3, load MOCVD device vaporization chamber after being well mixed；
C. system assembles：Vaporization chamber is connected with settling chamber by pipeline, is then placed in the good Mo substrate of advanced processing
In settling chamber, the assembling of system is completed；
D. the air-tightness for the system that argon gas checking step C is obtained is passed through, after confirming that system is air tight, argon flow amount is adjusted to
500ml/min ventilations 5min；
E. hydrogen is passed into settling chamber by pipeline, be then turned on induction heater to Mo substrate carry out sensing plus
Heat, Mo substrate is heated to required experimental temperature；
F. vaporization chamber heater, heating Ir (acac) are opened3；
G. after room to be evaporated is heated to required temperature stabilization, carried by argon gas by Ir (acac)3Gas (can be passed through altogether
Reacting gas) import settling chamber.Deposition starts, and absorbs tail gas using liquid cold-trap in deposition process；
H. after reaching predetermined sedimentation time, by Ir (acac)3Gas exports settling chamber, and closes in vaporization chamber and settling chamber
Between high-temperature valve, to stop Ir (acac)3Gas is then shut off vaporization chamber heater, so that evaporation to the conveying of settling chamber
Room carries out natural cooling.Power by adjusting induction heater slowly reduces the temperature of Mo substrate.When molybdenum base temperature is down to
After room temperature, H is closed successively2And Ar, open settling chamber and take out sample, clean settling chamber.
I. chemical method etching away Mo substrate is utilized, metal iridium is washed with deionized, then dries；
(2) high-temperature roasting prepares porous iridium：
In tube furnace, the metal iridium obtained to step (1) carries out high-temperature roasting.
SiC sand and Ir (acac) wherein in step (1) described in B3Ratio be 1：10 to 1：4.
Deposition chamber temperatures wherein in step (1) described in E, F are controlled at 460-540 DEG C, and vaporization chamber temperature control is in 250-
260 DEG C, to which the bright iridium coating layer of silvery white is made.
Coreaction gas described in G is the vapor that partial pressure is 606Pa wherein in step (1), it is therefore an objective to is decomposed with organic matter
Caused C reactions generation gas, avoids being attached to coating surface.Can also crystal grain thinning.Can be to the tail gas that is obtained in step G
In Ir (acac)3Recrystallized, can be used for reaction precursor below or for other purposes, to reach to Ir
(acac)3High usage；
Sedimentation time wherein in step (1) described in H is 180min.
The system of temperature-fall period wherein in step (1) described in H is：Cooling rate is 10 DEG C/min at more than 400 DEG C；
5 DEG C/min at 300-400 DEG C；Completely close heater at less than 300 DEG C, natural cooling, in order to avoid because thermal stress makes coating
Produce warpage.
Corrosive agent wherein in step (1) described in I is chloroazotic acid.
High-temperature roasting wherein described in step (2) is carried out in argon gas atmosphere.
High-temperature roasting heat treating regime wherein described in step (2) is：During heating：Programming rate is 10 at less than 800 DEG C
DEG C/min, soaking time 20min；5 DEG C/min at 800-1200 DEG C, soaking time 30min；3 DEG C during 1200-1500 DEG C/min/
Min, 60~420min of soaking time.During cooling：3 DEG C/min when 5 DEG C/min at 800-1200 DEG C, 1200-1500 DEG C/min,
Less than 800 DEG C furnace coolings.
The beneficial effects of the invention are as follows：Because iridium fusing point is high, fragility is big, therefore is difficult to according to generally preparing porous metals material
The method of material prepares porous iridium.The invention discloses a kind of new method for preparing porous iridium, have the advantage that：
(1) pore creating material or foams need not additionally be used, technological process is simple；
(2) after recycling acetic acid acetone iridium, presoma comprehensive utilization ratio is up to 80%；
(3) average pore size, the porosity of the porous iridium prepared can control.
Brief description of the drawings
Fig. 1 is porous iridium prepared by embodiment 1:Wherein (a) is EDS collection of illustrative plates, and (b) is SEM photograph；
Fig. 2 is porous iridium prepared by embodiment 2:Wherein (a) is EDS collection of illustrative plates, and (b) is SEM photograph；
Fig. 3 is porous iridium prepared by embodiment 3:Wherein (a) is SEM photograph.
Embodiment
The present invention will be further described with specific embodiment below in conjunction with the accompanying drawings：
Embodiment 1：A kind of method that two-step method prepares porous iridium, comprises the following steps：
1. the preparation of porous iridium
(1) mocvd method prepares iridium (Ir)：
Mo substrate is put into ethanol after blasting treatment and is cleaned by ultrasonic, scavenging period 10min, after cleaning
Matrix is put into baking oven and dried；By by the 5.8100g of recrystallization Ir (acac)3After being well mixed with 30g SiC powders
Load MOCVD device vaporization chamber；Vaporization chamber is connected with settling chamber by pipeline, and the good Mo substrate of advanced processing is placed in it is heavy
In product room；The air-tightness of argon gas inspection system is passed through, after confirming that system is air tight, argon flow amount is adjusted to 500ml/min ventilations
5min；Induction heater is opened after being passed through hydrogen, Mo substrate is heated to 480 DEG C；Vaporization chamber heater is opened, heats Ir
(acac)3To 255 DEG C；After room to be evaporated is heated to required temperature stabilization, carried by argon gas by Ir (acac)3Gas imports heavy
Product room.Deposition starts, and absorbs tail gas using liquid cold-trap in deposition process；After depositing 3h, by Ir (acac)3Gas export deposition
Room, and the high-temperature valve closed among vaporization chamber and settling chamber, close vaporization chamber heater.By the work(for adjusting induction heater
Rate slowly reduces the temperature of matrix:Cooling rate is 10 DEG C/min at more than 400 DEG C, 5 DEG C/min at 300-400 DEG C, 300 DEG C with
Heater, natural cooling will be completely closed when lower；When substrate temperature is down to room temperature, H is closed successively2And Ar, settling chamber is opened, is taken
Go out sample, clean settling chamber.Preparation chloroazotic acid, etching away Mo substrate, then cleaned and dried with deionized water.
(2) high-temperature roasting prepares porous iridium：
Sample is used into tube furnace, carries out high-temperature roasting under an argon atmosphere.During heating：Programming rate at less than 800 DEG C
For 10 DEG C/min, soaking time 20min；At 800-1200 DEG C DEG C/min, soaking time 30min；3 during 1200-1500 DEG C/min
DEG C/min, soaking time 300min.During cooling：3 DEG C/min when 5 DEG C/min at 800-1200 DEG C, 1200-1500 DEG C/min, 800
Furnace cooling below DEG C.
2. the detection of sample composition and micro-structural, characterize
(1) EDS (X-ray energy spectrum) analyses are carried out to porous iridium coating layer prepared by embodiment 1, as a result as the explanation of accompanying drawing 1. is heavy
It is long-pending to iridium coating layer in there is no other impurities element.
(2) accompanying drawing 1. is SEM (ESEM) photo of the porous coating prepared in embodiment 1, it can be seen that its aperture
Size is more consistent, and porosity is higher.By statistics, hole accounts for cross-section area ratio, and (the multiple different visual fields of selection are counted
Obtain average value) it is 11.15%.
Embodiment 2：A kind of method that two-step method prepares porous iridium, comprises the following steps：
1. the preparation of porous iridium
(1) mocvd method prepares iridium (Ir)：
Mo substrate is put into ethanol after blasting treatment and is cleaned by ultrasonic, scavenging period 10min, after cleaning
Matrix is put into baking oven and dried；By by the Ir (acac) of recrystallization35.6055g is filled after being well mixed with 30g SiC powders
Enter MOCVD device vaporization chamber；Vaporization chamber is connected with settling chamber by pipeline, and the good matrix of advanced processing is placed in settling chamber
In, the air-tightness of argon gas inspection system is passed through, after confirming that system is air tight, argon flow amount is adjusted to 500ml/min ventilations 5min；
Sensing heating is opened after being passed through hydrogen, matrix is heated to 480 DEG C；Open vaporization chamber heater, heating Ir (acac) to 255
℃；After room to be evaporated is heated to required temperature stabilization, carried by argon gas by Ir (acac)3Gas imports settling chamber, and is passed through
Vapor is as coreaction gas, partial pressure 606Pa.Deposition starts, and absorbs tail gas using liquid cold-trap in deposition process；Deposition
After 3h, by Ir (acac)3Gas and vapor export settling chamber, and the high-temperature valve closed among vaporization chamber and settling chamber, are closed
Vaporization chamber heater.Power by adjusting induction heater slowly reduces the temperature of matrix:Cooling rate at more than 400 DEG C
For 10 DEG C/min, 5 DEG C/min at 300-400 DEG C, heater, natural cooling are completely closed at less than 300 DEG C；Work as substrate temperature
Room temperature is down to, closes H successively2And Ar, settling chamber is opened, takes out sample, cleans settling chamber.Prepare chloroazotic acid, etching away molybdenum base
Body, then cleaned and dried with deionized water.
(2) high-temperature roasting prepares porous iridium：
Sample is used into tube furnace, carries out high-temperature roasting under an argon atmosphere.During heating：Programming rate at less than 800 DEG C
For 10 DEG C/min, soaking time 20min；At 800-1200 DEG C DEG C/min, soaking time 30min；3 during 1200-1500 DEG C/min
DEG C/min, soaking time 300min.During cooling：It is identical when more than 800 DEG C cooling rates are with heating, and without being incubated, 800 DEG C
Following furnace cooling.3 DEG C/min when 5 DEG C/min at 800-1200 DEG C, 1200-1500 DEG C/min, less than 800 DEG C furnace coolings.
2. the detection of sample composition and micro-structural, characterize
(1) EDS (X-ray energy spectrum) analyses are carried out to porous iridium coating layer prepared by embodiment 2, as a result as the explanation of accompanying drawing 2. is heavy
It is long-pending to iridium coating layer in there is no other impurities element.
(2) accompanying drawing 2. is SEM (ESEM) photo of the porous coating prepared in embodiment 2, it can be seen that its aperture
Size is more consistent, and porosity is higher.By statistics, hole accounts for cross-section area ratio, and (the multiple different visual fields of selection are counted
Obtain average value) it is 10.22%.Compared with Example 1, embodiment 2 is identical with its sedimentary condition, but due to being passed through vapor
Refined as coreaction gas, crystal grain refinement, hole.Because gaseous byproduct can be produced during coatings growth
Thing, this accessory substance will find passage effusion, so as to form gap between particle.If crystallite dimension is larger, because accessory substance is arranged
The gap gone out is difficult to be filled by it；When there is vapor to participate in reaction, the crystal grains fine of coating is small, and gap is easy to by little crystal grain
Filling, the coating for depositing to obtain is then relatively compact, and after heat treatment the ratio shared by coating inside aperture also diminishes.Embodiment 3：One
The method that kind two-step method prepares porous iridium, comprises the following steps：
1. the preparation of porous iridium
(1) mocvd method prepares iridium (Ir)：
Mo substrate is put into ethanol after blasting treatment and is cleaned by ultrasonic, scavenging period 10min, after cleaning
Matrix is put into baking oven and dried；By by the Ir (acac) of recrystallization35.7955g is filled after being well mixed with 30g SiC powders
Enter MOCVD device vaporization chamber；Vaporization chamber is connected with settling chamber by pipeline, and the good matrix of advanced processing is placed in settling chamber
In, complete the connection of pipeline；The air-tightness of argon gas inspection system is passed through, after confirming that system is air tight, argon flow amount is adjusted to
500ml/min ventilations 5min；Sensing heating is opened after being passed through hydrogen, matrix is heated to 520 DEG C；Open vaporization chamber heating dress
Put, heating Ir (acac) is to 255 DEG C；After room to be evaporated is heated to required temperature stabilization, carried by argon gas by Ir (acac)3
Gas imports settling chamber, and liquid cold-trap absorption tail gas is used in deposition process；After depositing 3h, by Ir (acac)3Gas export is heavy
Product room, and the high-temperature valve closed among vaporization chamber and settling chamber, close vaporization chamber heater.By adjusting induction heater
Power slowly reduces the temperature of matrix:Cooling rate is 10 DEG C/min at more than 400 DEG C, 5 DEG C/min at 300-400 DEG C, 300 DEG C
Heater, natural cooling are completely closed when following；When substrate temperature is down to room temperature, H is closed successively2And Ar, settling chamber is opened,
Sample is taken out, cleans settling chamber.Chloroazotic acid is prepared, etching away Mo substrate, is then cleaned and is dried with deionized water.
(2) high-temperature roasting prepares porous iridium：
Sample is used into tube furnace, carries out high-temperature roasting under an argon atmosphere.During heating：Programming rate at less than 800 DEG C
For 10 DEG C/min, soaking time 20min；At 800-1200 DEG C DEG C/min, soaking time 30min；3 during 1200-1500 DEG C/min
DEG C/min, soaking time 300min.During cooling：3 DEG C/min when 5 DEG C/min at 800-1200 DEG C, 1200-1500 DEG C/min, 800
Furnace cooling below DEG C.
2. the detection of sample composition and micro-structural, characterize
Accompanying drawing 3. is that SEM (ESEM) photos of the porous coating prepared in embodiment 3 and OM (metallographic microscope) shine
Piece, it can be seen that its pore size is more consistent, and porosity is higher.By statistics, hole accounts for cross-section area ratio, and (selection is multiple
Different visual fields carry out statistics and obtain average value) for 8.51%. compared with Example 1, the depositing temperature of embodiment 3 improves, finally
Hole occupied area reduces because the growth process of coating Hole is really coat inside defect in the mistake constantly assembled
Journey.The accumulation process of hole is the iridium coating layer Hole that is deposited at 520 DEG C as the crystal boundary migration in recrystallization process occurs
Shared ratio will integrally be less than the ratio shared by the coating Hole prepared at 480 DEG C.Because depositing temperature is higher, sink
Atomic migration ability enhancing during product, reduces coat inside defect, the compactness extent increase of coating.
Claims (10)
1. a kind of method that two-step method prepares porous iridium, it is characterised in that steps of the method are：
The first step, chemical vapour deposition technique prepare iridium, and detailed step is：
(1) Mo substrate is cleaned and dried；
(2) by SiC sand and Ir (acac)3Load vaporization chamber after well mixed；
(3) vaporization chamber is connected with settling chamber by pipeline, then the Mo substrate that step (1) obtains is placed in settling chamber, it is complete
Into the assembling of system；
(4) argon gas is passed into vaporization chamber by pipeline；
(5) hydrogen is passed into settling chamber by pipeline, is then turned on induction heater and sensing heating is carried out to Mo substrate；
(6) vaporization chamber heater is opened, to Ir (acac)3Heated；
(7) after room to be evaporated is heated to required temperature stabilization, carried by argon gas by Ir (acac)3Gas imports settling chamber, deposition
Reaction starts；
(8) after reaching predetermined sedimentation time, by Ir (acac)3Gas exports settling chamber, and closes among vaporization chamber and settling chamber
High-temperature valve, the heater of vaporization chamber is closed, then Mo substrate is cooled, after molybdenum base temperature is down to room temperature, successively
Hydrogen and argon gas are closed, sample is taken out from settling chamber；
(9) Mo substrate is eroded using the method for chemical attack, metal iridium and drying is then washed with deionized；
Second step, high-temperature roasting prepare porous iridium：
In tube furnace, the metal iridium obtained to the first step carries out high-temperature roasting.
2. the method that a kind of two-step method according to claim 1 prepares porous iridium, it is characterised in that：To molybdenum in step (1)
The process that matrix is cleaned and dried is：Mo substrate is put into ethanol after blasting treatment first and is cleaned by ultrasonic, is cleaned
Time is 10min, and matrix is put into baking oven after cleaning and dried.
3. the method that a kind of two-step method according to claim 1 prepares porous iridium, it is characterised in that：SiC sand in step (2)
With Ir (acac)3Mass ratio be 1：4-10.
4. the method that a kind of two-step method according to claim 1 prepares porous iridium, it is characterised in that：Step is passed through in (4)
The flow of argon gas is 500mL/min, and it is 5min to be passed through the time, so that vaporization chamber is in argon gas atmosphere.
5. the method that a kind of two-step method according to claim 1 prepares porous iridium, it is characterised in that：Adding in step (5)
Hot temperature is 460-540 DEG C.
6. the method that a kind of two-step method according to claim 1 prepares porous iridium, it is characterised in that：Adding in step (6)
Hot 250-260 DEG C of temperature.
7. the method that a kind of two-step method according to claim 1 prepares porous iridium, it is characterised in that：Step passes through in (7)
The gas of argon gas carrier band is Ir (acac)3The mixture of gas and vapor, the partial pressure of vapor is 606Pa in mixture.
8. the method that a kind of two-step method according to claim 1 prepares porous iridium, it is characterised in that：To molybdenum in step (8)
The program that matrix is cooled is：Cooling rate is 10 DEG C/min at more than 400 DEG C；5 DEG C/min at 300-400 DEG C；300 DEG C with
Induction heater, natural cooling will be completely closed when lower.
9. the method that a kind of two-step method according to claim 1 prepares porous iridium, it is characterised in that：It is chemical in step (9)
Corrosive liquid is chloroazotic acid used by the method for corrosion.
10. the method that a kind of two-step method according to claim 1 prepares porous iridium, it is characterised in that：Described in second step
High-temperature roasting is carried out in argon gas atmosphere, and described high-temperature roasting heat treating regime is：During heating：Heat up speed at less than 800 DEG C
Spend for 10 DEG C/min, soaking time 20min；5 DEG C/min at 800-1200 DEG C, soaking time 30min；1200-1500℃/min
When 3 DEG C/min, 60~420min of soaking time；During cooling：3 DEG C when 5 DEG C/min at 800-1200 DEG C, 1200-1500 DEG C/min/
Min, less than 800 DEG C furnace coolings.
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